1.
General Discussion
a. Principle: Filter a well-mixed sample through a standard glass-fiber filter. Then,
transfer the filtrate to a pre-weighed dish, evaporate it to dryness, and dry it to
constant weight in an oven at 180 2°C. The increase compared to the empty pre-
weighed dish weight represents TDS. These results may differ from the theoretical
value for solids calculated from chemical analysis of sample. Approximation methods
for correlating chemical and physical analyses are available.1 The filtrate collected
from the TSS determination (2540D) may be used to determine TDS.
To meet the LFB requirement (2540A.5), analysts can create a TDS standard as
follows: Dry NaCl at 103–105°C for 1 h, weigh 50 mg, and dilute to 1 L with reagent
water. This results in a 50-mg/L TDS standard.
b. Interferences: See 2540A.2. Highly mineralized waters with a considerable
calcium, chloride, magnesium, and/or sulfate content may be hygroscopic and require
prolonged drying, proper desiccation, and rapid weighing. Samples with high
bicarbonate concentrations require careful, possibly prolonged drying at 180 2°C to
ensure that bicarbonate completely converts to carbonate. Residues dried at 180 2°C
will lose almost all mechanically occluded water, but some water of crystallization
may remain, especially if sulfates are present. Organic matter may volatilize and be
lost, but not completely removed. CO2 loss occurs when bicarbonates convert to
carbonates, and carbonates may be decomposed partially to oxides or basic salts.
Some chloride and nitrate salts may be lost. In general, evaporating and drying water
samples at 180 2°C yields TDS values closer to those obtained by adding individually
determined mineral species than the values obtained when drying at 103–105°C.
Because excessive residue in the dish may form a watertrapping crust, limit sample to
200 mg residue.
2. Apparatus
Apparatus listed in 2540B.2a–l, and in addition:
a. Glass-fiber filter disks, 22 to 125 mm dia, 2-m nominal pore size without
organic binder.*
b. Filtration apparatus: One of the following, suitable for the filter selected:
1) Membrane filter funnel—various capacities, to fit selected filter.
2) Gooch crucible—25- to 40-mL capacity, with Gooch crucible adapter.
3) Filtration apparatus with reservoir and coarse (40- to 60-m) fritted disk as filter
support.†
c. Suction flask with sufficient capacity for sample size selected.
d. Oven that operates at 180 2°C.
3. Procedure
a. Preparation of glass-fiber filter disk: Insert disk with wrinkled side up into
filtration apparatus. Apply vacuum and wash disk with three successive volumes
of 20 mL reagent-grade water. Continue suction to remove all traces of water. If
using commercially prepared glass-fiber filter disks, the washing step may be
skipped if the manufacturer certifies that the filters meet this method’s
requirements.
b. Preparation of evaporating dish: If measuring volatile solids, ignite cleaned
evaporating dish at 550 50°C for 15 min in a muffle furnace. If only measuring
TDS, then heat cleaned dish to 180 2°C for 1 h in an oven. Cool dishes to ambient
temperature and weigh. Store in desiccator or oven until needed.
c. Selection of filter and sample sizes: Choose sample volume to yield between 2.5
and 200 mg dried residue. If filtration will take 10 min to complete, then increase
filter size or decrease sample volume. Identify any sample that yields residue 2.5
mg or 200 mg, and report the value as described in Sections 1020 and 2020.
d. Sample analysis: Stir or mix sample and use a pipet or graduated cylinder to
transfer a measured volume onto a glassfiber filter with applied vacuum. Wash the
entire exposed surface of filter with three successive volumes of 10 mL reagent-
grade water. Allow complete drainage between washings, and continue suction
until all traces of water are removed. Transfer total filtrate (with washings) to a
pre-weighed evaporating dish and evaporate to dryness on a steam bath, hot plate,
or block, or in a drying oven. If necessary, add successive portions to the same
dish after evaporation. Dry evaporated sample for 1 h in an oven at 180 2°C, cool
in a desiccator to ambient temperature, and weigh. Repeat cycle (drying, cooling,
desiccating, and weighing) until weight change is 0.5 mg. If determining volatile
solids, follow procedure in 2540E.
4. Calculation
( A−B )∗1000
mg total dissolved solids/L =
sample volume ,mL
where:
A final weight of dried residue dish, mg, and
B weight of dish, mg.
5. Precision
Single-laboratory analyses of 77 samples of a known of 293 mg/L were made with
a standard deviation of differences of 21.20 mg/L.
6. Reference
1. SOKOLOFF, V.P. 1933. Water of crystallization in total solids of water
analysis. Ind. Eng. Chem., Anal. Ed. 5:336.
7. Bibliography
HOWARD, C.S. 1933. Determination of total dissolved solids in water
analysis. Ind. Eng. Chem., Anal. Ed. 5:4.
U.S. GEOLOGICAL SURVEY. 1974. Methods for Collection and Analysis of
Water Samples for Dissolved Minerals and Gases. Techniques of
Water-Resources Investigations; Book 5, Chap. A1. Washington,
D.C.
